Hydrochloric Acid → HCID 89462848, 화합물

HRID 1473254노트

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HRID 1473254 반응식
[F:1][C:2]1[CH:25]=[CH:24][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]([C:16]([O:18]C)=[O:17])=[C:8]2[C:20]([O:22]C)=[O:21])=[CH:4][CH:3]=1.[OH-].[K+].Cl>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]([C:16]([OH:18])=[O:17])=[C:8]2[C:20]([OH:22])=[O:21])=[CH:24][CH:25]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 89462967HCID 89462967, 화합물

생성물 1

HCID 89462848HCID 89462848, 화합물수율 86.3%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
95 °C

실험 절차

A rbf charged with dimethyl 1-(4-fluorobenzyl)-1H-indole-2,3-dicarboxylate (3.79 g, 11.10 mmol) was treated with a solution of KOH (7.48 g, 133 mmol) in Ethanol (13.88 ml) (0.5 M solution) and heated to reflux (95° C. bath temp). After 18 h, the reaction mixture was cooled to ambient temperature, and acidified to pH 1 with 4M HCl and extracted with EtOAc. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated to afford 1-(4-fluorobenzyl)-1H-indole-2,3-dicarboxylic acid (3.0 g, 9.58 mmol, 86% yield) as a yellowish solid. LCMS (m/z) ES+=314 (M+1).

후처리

  1. temperatureheated
  2. temperaturethe reaction mixture was cooled to ambient temperature
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e98d88eb99514744be2708b81d4d406b
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012642B2

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